2-[(6-氯-3,4-二氢-3-甲基-2,4-二氧代-1（2H）-嘧啶）甲基]丁苯甲腈合成路线 （共 7 条）
反应条件
1: 2-((6-chloro-2,4-dioxo-3,4-dihydropyrimidin-1(2H)-yl)methyl)benzonitrile With sodium hydride; lithium bromide in tetrahydrofuran; N,N-dimethyl-formamide T=20°C; 0.333333 h; 2: methyl iodide in tetrahydrofuran; N,N-dimethyl-formamide T=0 - 35°C; Further stages.;
参考文献
Feng, Jun; Gwaltney, Stephen L.; Stafford, Jeffrey A.; Zhang, Zhiyuan; Brodluahrer, Paul R.; Elder, Bruce; Isbester, Paul; Fornicola, Richard S.; Kisanga, Philip B.; Mobele, Bingidimi I.; Palmer, Grant J.; Reeve, Maxwell M.; Salsbury, Jonathon S.; Ulysse, Luckner; Venkatraman, Sripathy
Patent: US2009/275750 A1, 2009 ;
Location in patent: Page/Page column 22 ;
US 20090275750 A1
反应条件
1: 2-((6-chloro-2,4-dioxo-3,4-dihydropyrimidin-1(2H)-yl)methyl)benzonitrile With sodium hydride; lithium bromide in tetrahydrofuran; DMF (N,N-dimethyl-formamide) T=0 - 20°C; 0.333333 h; 2: methyl iodide in tetrahydrofuran; DMF (N,N-dimethyl-formamide) T=20 - 35°C;
参考文献
Andres, Mark; Lorimer, Keith
Patent: US2007/66635 A1, 2007 ;
Location in patent: Page/Page column 13-14; 14 ;
反应条件
N-ethyl-N,N-diisopropylamine in 1-methyl-pyrrolidin-2-one T=0 - 70°C; Inert atmosphere;
参考文献
US2009/275750 A1, ;
Page/Page column 23 ;
US 20090275750 A1
反应条件
1: With trichlorophosphate T=0°C; 2: With water T=0 - 110°C;
参考文献
MAPI PHARMA HK LIMITED; MAROM, Ehud; MIZHIRITSKII, Michael; RUBNOV, Shai
Patent: WO2010/109468 A1, 2010 ;
Location in patent: Page/Page column 25-26 ;
反应条件
phosphorus pentachloride; N-benzyl-N,N,N-triethylammonium chloride; trichlorophosphate in acetonitrile 4 - 5 h; Reflux; Product distribution / selectivity;
参考文献
MAPI PHARMA HK LIMITED; MAROM, Ehud; MIZHIRITSKII, Michael; RUBNOV, Shai
Patent: WO2010/109468 A1, 2010 ;
Location in patent: Page/Page column 26 ;
反应条件
1.1: NaH / dimethylformamide; dimethylsulfoxide / 0.5 h / 0 °C 1.2: LiBr / dimethylformamide; 1,2-dimethoxy-ethane / 0.25 h / 0 - 20 °C 1.3: 54 percent / dimethylformamide; dimethylsulfoxide / 0 - 20 °C 2.1: NaH; LiBr / dimethylformamide; tetrahydrofuran / 0.33 h / 20 °C 2.2: 72 percent / dimethylformamide; tetrahydrofuran / 0 - 35 °C View Scheme
参考文献
Journal of Medicinal Chemistry, , vol. 50, # 10 p. 2297 - 2300
反应条件
sodium hydrogencarbonate in methanol T=100°C; 2 h; Molecular sieve;
参考文献
Takeda San Diego, Inc.
Patent: EP1586571 A1, 2005 ;
Location in patent: Page/Page column 43-44 ;
